Manufacture of cream of tartar.



of Switzerland, residing,

lo the following is a specification.

45 operating UNTTED ETATEE PATENT @FlElUOE HUMBERT CANTONI, OF VOGHERA,ITALY, JEAN CHAUTEMS AND EMILE DEGRANGE, OF GENEVA, SWITZERLAND,ASSIGNORS TO THE FIRM 0]? CAN- TONI' CHAUTEMS ET COMPAGNIE AND EMILEDEGRANGE, 0F GENEVA,

SWITZERLAND. v

MANUFACTURE OF CREAM OF TARTAR.

No Drawing.

To all whom it may concern Be it known that we, IIUMBERT (borrow, asubject of the King of Italy, and JEAN CIIAUTEMS and EMILE DEGRANGE,citizens respectively, at

Voghera, Italy, and Geneva, in the Confederation OIE Switzerland, haveinvented certain new and useful Improvements in the Manufacture of Creamof Tartar, of which The present invention relates to a. process forextracting and recovering in the torm of potassium bitartrate (cream oftartar) the whole of the tartaric acid which is contained in the lees ofwine, crude tartar or argol, residues of the distillation of stillcrystals, wine, calcium tartrate or any other tartaric materialwl-iatsoever.

The processes known heretofore, according to which the cream of tartaris obtained by\ precipitation, all possess the defect or disadvantagethat the employment of large quantities of dissolving and precipitatingagents is necessary. In these processes the raw materials are'attackedeither by means of an acid and the potassium bitartrate is precipitatedfrom the solution obtained by means of an alkaline reagent or the rawmaterial is treated with an alkaline agent,

wher'eaftcr the potassium bitartrate is precipitated fromv its solutionby means of an acid. In both the cases the precipitation takes place inthe presence of a suitable quantity of a potassium salt. In the first-case it is possible to operate in the cold,

while in the second case heat has to be eniployed, in order to decomposecompletely the raw material, when the same contains calcium 'tartrate.It has now been shown that '40 an important saving of combustible matterand especially ,of reagents may be obtained by treating the rawmaterial, instead of either only with an acid or alkaline agent, in asuitable manner with the two agents by either successively upon a singleportion of the material, or separately or separately and successivelyupon several portions of the raw materials, in order that the alkalineagent converts the potassium bitar- '50 trate, which is contained in theraw material,

wholly or according to the composition of the raw material and theoperative method Specification of Letters Patent.

Patented July 14, 1914i.

Application filed February 8, 1912. Serial No. 676,449.

employed, only partly into a normal tartrate, for instance, Seignettesmore soluble than cream of tartar,- this -salt being dissolved, and thatthe acid agent dissolves the calcium tartrate, when such is present,whichgenerally is the case, and ac-, cording to the method employed thewhole of the cream of tartar or only the; rest of the same whicheventually has not been transformed by the alkaline agent, "by formingfree tartaric acid and the potassium and calcium-salts of the acidemployed. In this manner two solutions, one an alkaline and the other anacid, are obtained, which are ,mixed together after the calculatedamount of a potassium-salt has been added to the alkaline solution andthe calculated amount tartaric acid which was originally contained ascalcium tartrate in the raw material, into potassium bitartrate, and onthe othcr hand the Whole of the calcium contained in the acid solutioninto insoluble calcium oxalate. By mixing and stirring the two solutionstogether the Whole tartaric acid contained in the raw materialprecipitates in form of potassium bitartrate mixed with calcium oxalateand is separated'from the latter by means of boilingwater to which alittle oxalic acid has been added, wheroaitter the solution isdecolorizcd and the cream oftartar crystallized. Such a process formsthe subject of the present invention. The advantage which it offers ascompared with the known process is easily shown from the followingcomparison of the different processes in which, because of thesimplicity, it is supposed that theraw materials do not contain anycalcium tartra'te.

A. Treatment of the raw material with on acid agent and precipitation ofcream of tartar from the acid solution by means of cor/alkaline reagent.

1. Solwtioa- 2C O H KH+2HCl:QQ'O H -{QKCI. 2. Precipitation of orozim oftartar that is to say: by using two molecules 'HCl salt, which is,

and one molecule CO Na one obtains two molecules cream of tartar.

B. Treatment of the raw materials 'withan alkaline agent andprecipitation 0 f the cream of tartar from the alkaline solution.

by means of an aeicl.

1. Solati0n 2. Precipitation 07' ereant'of tarta11 QQUJLIiNa-l-QHCI: I

2C O H KH+2NaCl that is to say one obtains by employing one molecule (10N21 and two molecules HCl again two molecules cream of tartar.

0. Treatment of the raw materials accordinfl to the present inventionwith (In-alkaline ancl an acid magent and precipitation.

A that is to say one obtains by the employment.

5 of one molecule (10 N51 and two-molecules HCl four molecules cream oftartar.

When the raw materials contain calcium tartrate,which is generally theease, the re actions pass in a similar manner after addition of oxalicacid to the acid and a potassium salt, for instance potassium chlorid,to the alkaline solution:

Here it is to be observed that each tartrate is treated with the mostsuitable dissolvent phases and wholly in namely the postassiumbitartrate, with carbonate of sodium and the calcium tartrate withhydrochloric acid.

2. l reeipitationaftet' additionof potassium chlorirl t0 the alkalineand omalio acid to the acitl solution/ 2CaCl +2C O H =2C O Ca+4HCl (3C,OILKNa+2C O H +4HCl+2KCl:

. 8C O H KH+6NaCL These two reactions take place simultaneously andarerep'resented by separate equa tions for the sakeof clearness.

of tartar. practice to employ oxalic acid or oxalates l'Vith a smallerproportion of calcium tartrate one would for example have:

phases wholly. in the have not heal attacked by I the carbonate ofsodium.

. 100 0 1] +4CaCl +6KCL Preeipitation.One has Sill'lllllltllGOHSl y4CaCl +4Q OJI :4C,O Ca+8HCl 18C,O H ,KNa 100 0 11 SHCl 6KC1 (coming fromthe raw materiirU-HLKGI en added) Q8C O ILKH+ (which has be 18NaCl. 7

Owing to the combined treatment of the raw materials'with alkaline andacid agents and to the following nnxing of the obtalned solutions thereresults the. advantage that,

even. w en exactly the same proportions of reagents are employed for theattack of the raw materials, by the same total employment of reagentsone dissolves twice as much tartariccompounds as compared with theprocesses hitherto known. Therefore the double amount ot-crcam of tartarcan be ob tained. In this manner the Working-expenses are reduced in alarge proportion and an economy of 50% of reagents is ol'itained. Sinceall the reactions can be carried out wholly in the cold, there is as aresult the economy of fuel I 7 It is well known by us thatv hioxalate ofpotassium is employed for refining cream Herctolore it has also been theand potassium salts in connection with the production of cream of tartarvfrom crude materials containing calcium ta rtrate. However, accordingto this practice the crude material was directly subjected to the actionof hot water to whichoxalic acid or oxalates were added in quantityabout equivalent to the calcium tartratc present and the mixture boiledin presence of a sufficient quantity of potassium chlorid or otherpotassium salt for converting the calcium tartrate into bitartrate ofpotassium and calciumoxalate. As a result, a considerable quantity ofboiling Water and rel atively .niuch time are required. The calciumoxalate obtained remains in the residues. 'In contradistinction thereto,the oxalic acid and the potassium salt are,ac -.ord

ing to the present invention, only employed,

after the acid and alkaline solutions are prepared and they are added tothe respective solutions in; the cold and in such quantitles, that onthe-one hand the Ca which ment, in order cium tartrat'e,

is contained in the acid solution as CaGl is precipitated in the form ofcalcium oxa late and on the other hand the free tartaric acid of theacid solution which originally existed as ealcium-tartrate, isprecipitated together with the tartaric acid which existed originally aspotassium bitartrate, in the form of cream of tartar.

The separation of the calcium-oxalate from the cream oftartar -by meansof boiling water, and also the regeneration .of the oxalic acid from thecalcium .oxalate present no difliculties whatsoever. For the presentprocess the alkaline reagents which are employed may advantageouslyconsist of aqueous solutions of carbonate "of sodium or potassium,ammonia and the like. As acid reagents, diluted acids such as forexample hydrochloric acid, sulfuric acid and the like, may be employed.These reagents are advantageously refined before their employthat theyshall not contain any noxious matters such as for example lead. arsenic,iron, etc., which would spoil the cream of tartar.

This process may following as Example N0. 1.

be illustrated by the 100 kg. lees of wine containing 25% tartaric acid,22% of which being in form of potassium bit-artrate and 3% in form ofcalare divided after. being crushed and torrefied, in tanks arranged oneabove the other in cascade fashion and treated in the cold with anaqueous solution of 8 kg. sodium carbonate of 9798% which is poured-bysmall portions into the highest tank. The reaction being finished inthis tank, the liquid iscaused to flow successively into the lowertanks. The residue is washed at first with the last alkalinewashing-liquor of a preceding treatment oftartaric material and atlastwith pure water. Thereafter the residue resulting from the treatmentof the raw material with the solution of sodium carbonate is'treated ina similar manner as above mentioned and also in the cold with 31 litersof hydro chloric acid of9 degrees Baum. The insoluble residue is alsotreated at first with the last acid washing liquors of a precedingtreatment and finally with pure water. The two first alkaline and acidwashing liquors are added respectively to the alkaline and the acid mainsolution. Then 3 kg. oxalic acid are added to the acid and 1.7 to 1.8kg. potassium chlorid'to the alkaline solution. These two solutions arenew mixed together under continuous stirring, wherebypotassiumbitartrate and calcium-oxalate precipitate. The solution isdecanted and portions thereof mixed respectively with sodium carbonateand hydrochloric acid, so that said solution can be reemployed for thetreattreating two exactly of the one quantity ment of crude material.The remaining portion of this solution may be also employed for thefirst. washing of the residue of the following attack of crude material.The precipitate consisting of cream of tar: tar and calcium oxalateafter having been centrifugally separated from the solution, is at firstwashed with cold water and then treated with about 600 litersof boilingwater, to which 3300 grams oxalic acid have been added, in. order toextract the cream of tartar. The calcium oxalate remains in a solidstate and the solution of cream of tartar is decanted from thecalcium-oxalate, decolorized by means of animal-charcoal or anotherdecolorizing reagent and filtered while still hot. The cream of tartarcrystallizes out of the filtered solution. The crystalsobtained are ofthe maximum purity and contain as shown by analysisfroin be-, tween 99.7to 100% potassium bit-artrate. The calcium oxalate which remains in asolid state is employed for regenerating the' oxalic acid. The samecycle of operations can also be realized and the same chemical andeconomical results can be obtained by calculated quantities of the samecrude material or of two different crude materials independently of eachother until there is obtained complete extraction with one or morealkaline agents in the cold or the heat and of the other with one ormore acid agents in the cold. The quantities of the reagents and ofthe'crude materials employed are calculated in such a manner that bymixing the two alkaline and acid solutions the same chemical andeconomical result is obtained as that obtained by operating in the abovedescribed first manner. The chemical reactions which take place in thiscase may be represented by the following equations:

1. Treatment of one portion of the crude mmte'rial with an acid reagent-Treatnwnl oftha other portionof the crude malarial with an (tlhalznereaganl--' in the presence of .heat or in the cold, de pending uponwhether or not any calcium tartrate is present.

3-3 tion of a normal tartrate, and a.

This method of the process is advantageously employed 1n the case Wherecrude materials containing no calciumtartrate and materials which, onthe contrary, are :jvery l'lCll in calcium tartrate, have to be treatedsm'lultanctmsly. 1 This case may be illustrated by the iollowlng as:

' Eacample N0. 2.

it) On the one hand 90 kilograms crude tartar containing 80% potassium.bitartrate are treated with an aqueous solution of 29 kg.

carbonate of sodium of 97-98% and on the other hand 100 kg. lees of Winecontaining 26% tartaric acid, 1.8% of which being in 1. The hereindescribed process for (BX-- 130 trawling and recovering in the form ofpotassiuln bitartrate all the tartaric acid contained in tartaricmaterials, consisting in (treating raw tartaric materials by means ofalkaline and. acid agents to obtain a solusolution of tree tartaricacid, and then mixing the said solutions together to precipitate ascream .ot' tartar all the tartaric acid contained,

therein.

The herein described process for extracling and recovering in the formof cream 01" tartar all of the tartaric acid containcd in tarta icmaterials consisting in treating 'a portion of thecrude materials with45 alkaline reagents to obtain a solution of a normal tartrate, treatinganother portion of the crude materials with acid reagents to obtain asolution of free tartaric' acid, and then mixiz'ig the two solutionstogether to precipitate as cream of tartar the Whole tartaric acidcontained therein.

3. The herein described process for ,,ex

tracting and recovering in the form of cream tain a. solution of anormal ta-rtrate, treatinganother portion of the crude material withacid reagents "to obtain a solution of free tartaric acid, and thenmixing the two solutions together to precipitate as cream of tartar allthe tartaric acid contained therein.

l. The herein described process of-extractmg and recovering n the formof potassium bitartrate all .the tartaric llCldCOIltiLlIlBCl 1n tartaricmaterials consisting in treating raw tartaric'materials by means ofalkline and acid agents to" obtain a solution of'normal, tartrate and asolution of free tartaric acid, adding a potassium salt to the alkalinesolution, adding oxalic acid to the acid solution, and then mixing thesaid solutions together to precipitate as cream of tartar all thetartaric acid contained therein.

5. The. herein described process of extracting and recovering in theform of potassium bitartrate all of the tartaric acid contained in t1'taric materials, consisting in first treating a portion of the crudematerials with alkaline reagents to obtain the solution of normaltartrate, adding a potassiumv salt to this alkaline solution thentreating another portion of thecrude materials with-- acid reagents toobtain a solution of free tartaric acid, adding a predetermined quantityof oxalic acid to thls acid solution, and then mixing the two solutionstogether to precipitate as cream of tartar all the tar t'aric aci lcontained therein.

In testimony whereof We have aflixed our signatures in presence of twowitnesses. v

-- HUlVIBER-T CANTON-I.

JEAN CHAUTEMS. EMILE DEGRANGE. lVitnesses:

RonoLrnn on \Vunsrnamnno, Tmionomc IMER.

